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BCIS-02 REV.

BCI Battery
Technical FEB02
Manual

Issued 1992-03
Current Revision: 2002-02

RECOMMENDED TEST PROCEDURES FOR BATTERY MATERIALS

TABLE OF CONTENTS
1. Material Requirements .............................................................................................................. 3
2. Standard Specifications for Pig Lead ........................................................................................ 3
3. Hard Rubber .............................................................................................................................. 4
3.1. Rubber Containers .................................................................................................................... 4
3.2. Rubber Covers. ......................................................................................................................... 6
4. Plastic ........................................................................................................................................ 6
4.1. Raw Material Resin ................................................................................................................... 6
4.2. Plastic Containers...................................................................................................................... 8
4.2.1. Acid Resistance Tests ............................................................................................................... 9
4.2.2. Impact Resistance.................................................................................................................... 11
4.2.3. Bulge Test ................................................................................................................................ 13
4.2.4. Electrical Breakdown` .............................................................................................................. 13
4.2.5. Adhesion .................................................................................................................................. 14
4.2.6. Tensile Pull Test for Side Terminals ........................................................................................ 14
4.2.7. Torque Test for Side Terminals ............................................................................................... 16
4.2.8. Leakage Test for Side Terminals ............................................................................................. 17
4.3. Plastic Covers.......................................................................................................................... 18
4.3.1. Acid Resistance ....................................................................................................................... 18
4.3.2. Impact Resistance.................................................................................................................... 18
4.3.3. Bushing Impact Resistance ..................................................................................................... 19
4.3.4. Bushing/Stud Torque Test ....................................................................................................... 19
4.3.5. Adhesion. ................................................................................................................................. 20
5. Separator Test Methods .......................................................................................................... 20
5.1. Test I – Ohmic Resistance ...................................................................................................... 20
5.1.1. Procedure IA – Pre-Treatment................................................................................................. 20
5.1.2. Procedure 1B – Ohmic Resistance.......................................................................................... 21
5.2. Test II – Dimension Measurement .......................................................................................... 30
5.2.1. Procedure IIA – Height and Width ........................................................................................... 30
5.2.2. Procedure IIB – Squareness.................................................................................................... 31
5.2.3. Procedure IIC – Backweb Thickness ....................................................................................... 31
5.2.4. Procedure IID – Overall Thickness .......................................................................................... 32
5.3. Test III – Determination of Volume Porosity............................................................................ 34
5.4. Test IV – Determination of Pore Size Distribution ................................................................... 35
5.5. Test V – Analyses for Impurities and Acid Extractables.......................................................... 36
5.5.1. Procedure VA – Acid Extraction............................................................................................... 36
5.5.2. Procedure VB – Chloride Analysis........................................................................................... 37
5.5.3. Procedure VC – Metal Analysis ............................................................................................... 39
BCIS-02 Rev. Feb02

5.6. Test VI – Stiffness Measurement ............................................................................................ 39


5.7. Test VII – Determination of Puncture Resistance ................................................................... 41
5.7.1. Procedure VIIA – Globe Tester................................................................................................ 41
5.7.2. Procedure VIIB – GNB (“Gould”) Puncture Tester................................................................... 43
5.8. Test VIII – Wetting Properties.................................................................................................. 44
5.8.1. Procedure VIIIA – Acid Flotation Method................................................................................. 44
5.8.2. Procedure VIIIB – Acid Drop Absorption Method .................................................................... 45
5.8.3. Procedure VIIIC – Dry Charge Process Simulation ................................................................. 45
6. Sealing Compound .................................................................................................................. 46
7. Electrolyte ................................................................................................................................ 47
8. Intercell Connectors................................................................................................................. 48
9. Post Straps .............................................................................................................................. 48
10. Plates....................................................................................................................................... 48
11. Handles.................................................................................................................................... 48
12. Tapered Terminal Posts .......................................................................................................... 48
13. Side Terminals......................................................................................................................... 49

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1. MATERIAL REQUIREMENTS

1.1. Materials Not Described

Unless otherwise detailed in this specification, all material used in the construction of
batteries shall conform to best commercial practices. Active material, grid alloy or
miscellaneous lead parts smelted from other batteries must be refined prior to subsequent
use in new batteries.

2. STANDARD SPECIFICATIONS FOR PIG LEAD

ASTM Designation B29-79(84). This standard covers pure lead of two grades for use in
producing oxide for active material or alloying with various materials for grid alloys. The
chemical requirements are shown in Table I.

Table I
Chemical Requirements %

Corroding Common
Element Lead Lead
Silver (max) .0015 .005
Copper (max) .0015 .0015
Silver & Copper (together) .0025 -
Antimony, Arsenic, Tin (Together, max) .002 .002
Zinc (max) .001 .001
Iron (max) .002 .002
Bismuth (max) .050 .050
Lead (by difference) 99.94 99.94

2.1. BCI Standard Reference Materials

Standard Reference Materials have been developed by the BCI Technical Committee for use
by lead and battery manufacturers. Materials exist for 1, 3, and 6% antimony as well as lead-
calcium-aluminum alloys with and without tin. The analyses of these materials are shown in
Table II.

Table II
Chemical Analyses of BCI Standard Reference Materials
Material Designation

Element 1 3 6 CA CS
Aluminum <.0005 <.0005 <.0005 .019 .018
Antimony 1.08 2.70 5.98 <.0003 <.001
Arsenic 0.136 .151 .169 <.0003 <.0005
Bismuth 0.0103 .0073 .0046 .0105 .010
Calcium <.0005 <.0005 <.0005 .111 .085
Copper 0.0107 .053 .057 .0003 .0004
Iron <.0003 <.0003 <.0003 <.0003 <.0005
Nickel .0003 .0004 .0004 <.0002 <.0002
Selenium .0142 <.0005 <.0005 <.0002 <.0001
Silver .0018 .0012 .0010 .0017 .0017
Sulfur .0015 .0037 .0037 <.0005 <.0005
Tin .19 .165 .306 <.001 .272
Tellurium <.001 <.001 <.002 <.0003 <.0001

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Zinc <.0003 <.0003 <.0003 <.0005 <.0003

These materials are available from RSR Corporation, 1111 West Mockingbird Lane, Dallas,
TX 75257, Attn: R. D. Prengaman.

3. HARD RUBBER

3.1. Rubber Containers

The containers when tested in accordance with ASTM procedure designated D639-60-T,
entitled “Tentative Methods of Testing Battery Containers Made From Hard Rubber or
Equivalent Materials” revised 1960 shall meet the following chemical, electrical and physical
requirements:

3.1.1. Manganese (maximum) 0.003%

3.1.2. Iron (maximum) 0.3%

3.1.3. Acid Resistance

(a) Exact Days of Immersion ......................... 28 days


(b) Change in Dimensions (maximum).......... 2%
(c) Change in Weight (maximum).................. 35 mil. per sq. inch
(35 mil per 6.45 cm2)
(d) Acid Penetration (maximum).................... 1/64 inch (.40 mm)

3.1.4. Impact Resistance

3.1.4.1. 2.0 lb. ± 0.05 lb. (907 g ± 23) Solid Steel Ball shall be used. Impact Points shall be as shown
on Figure A. First impact point choice is exactly at H/2, however, if embossed letters, design
bands, etc. interfere, the impact point may be between H/3 and H/2, at a point of minimum
wall thickness. (Note that impact point is always on the center line of the cell).

3.1.4.2. Number of Points to be impacted, as shown on Figure A.

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Figure A. Impact Points for Various Configurations

3.1.4.3. Two averages will be compared with the following values, as well as the lowest single value
for each span. The short span will be averaged (12 values in the case of a 12V “S”
assembly), and the long spans will be averaged (2 values in the case of a 12V “S” assembly).
The following impact values must be met:

Minimum Impact
Battery Service Resistance
1. 6V and 12V passenger 12 in.-lb. Average for short spans
car and light 12 in.-lb. Average for long spans
commercial plus 30H No impact value below
and 30 HR. 8 in.-lb.

2. 6V and 12V heavy 20 in.-lb average for short spans


duty commercial motor 20 in.-lb average for long spans
coach and bus except No impact value below
30H and 30 HR. 16 in.-lb.

3.1.5. Bulge Test

(a) Water Temperature ..............160°F ± 2.0°F (71.1°C ± 1.1°C)


(b) Bulge Characteristics............No value greater than .070 in. (1.78 mm)

3.1.5.1. Hot-Cold Cycles

No failures permitted on 10 cycles

3.1.6. Electrical Breakdown Test

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(a) Test voltage shall be 100V per mil. thickness based on minimum thickness of container as
specified in the container design drawing, and not to exceed a maximum of 30,000V
(alternating peak voltage) applied between the electrodes.

(b) No failures permitted in the sample lot (See Tech. Con Rec.)

3.2. Rubber Covers

Chemical, physical, electrical and compound adhesion requirements shall be the same for
covers as for containers.

4. PLASTIC

Table 1
Plastic Test Reference
4.1 Raw Material Resin 4.1.1 Metal Impurities (Leach Method)
4.1.2 Accelerated Heat Aging
4.2 Plastic Containers 4.2.1 Acid Resistance Tests
4.2.2 Impact Resistance
4.2.3 Bulge Test
4.2.4 Electrical Breakdown
4.2.5 Adhesion
4.2.6 Tensile Pull Test for Side Terminals
4.2.7 Torque Test for Side Terminals
4.2.8 Leakage Test for Side Terminals
4.3 Plastic Covers 4.3.1 Acid Resistance
4.3.2 Impact Resistance
4.3.3 Bushing Impact Resistance
4.3.4 Bushing/Stud Torque Test
4.3.5 Adhesion
Physical tests should be done on components no less than twenty-four (24) hours after
molding at room temperature.

4.1. Raw Material Resin

4.1.1. Metal Impurities (Leach Method) Acid Reflux Analysis

4.1.1.1. Scope

This procedure provides a method for extracting acid soluble contaminants from
polypropylene molding resin by refluxing in sulfuric acid followed by analysis for metallic
impurities.

4.1.1.2. Apparatus

4.1.1.2.1. 250 ml Erlenmeyer flask with standard 24/40 ground glass joint

4.1.1.2.2. Reflux condenser with joint

4.1.1.2.3. Thermostat-controlled hot plate.

4.1.1.2.4. Balance capable of weighing to an accuracy of ± 0.025% of applied load.

4.1.1.2.5. Sulfuric acid (1.265 sp. gr. 80/80) – J. T. Baker, Trace Metal Analytical Grade or equivalent

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4.1.1.2.6. Deionized Water

4.1.1.2.7. Scissors

4.1.1.2.8. 500 ml. Volumetric flask

4.1.1.2.9. Filter unit with 0.45 micron membrane

4.1.1.2.10. Spectrometer-ICP (Inductively Coupled Plasma), AA (Atomic Absorption) or equivalent.

4.1.1.3. Procedure

4.1.1.3.1. Accurately weigh 10.0 g. ± 0.1 g. of clean (Deionized Water rinsed), dried polypropylene resin
material; either pellets or molded parts (molded parts should be cut into approximately 0.25
cm (0.1 in.) cubes). Sample to be dried at 100ºC - 115ºC (212°F – 239°F) for one hour.

4.1.1.3.2. Transfer the weighed material to the 250 Erlenmeyer flask and add 100 ml of 1.265 sp. gr.
80/80 sulfuric acid.

4.1.1.3.3. Attach reflux condenser, mount on hot plate, heat rapidly to boil and adjust rate to one drop
per second.

4.1.1.3.4. Prepare one (1) blank (control sample), reflux assembly, as noted above (4.1.1.3.2-3) without
polypropylene molded resin.

4.1.1.3.5. Both samples should be boiled for five (5) hours and allowed to cool to room temperature.

4.1.1.3.6. Filter solutions through the filter unit.

4.1.1.3.7. These extracts are now ready for analysis.

4.1.1.3.8. Quantitative elemental analysis should be performed in accordance with the ICP
manufacturer’s recommendations using the standards and prepared samples described
above. Alternative methods such as atomic absorption or x-ray fluorescence may be
substituted in the absence of an ICP.

4.1.2. Accelerated Heat Aging (Molded Plaques) Oven Oxidation Test

4.1.2.1. Scope

This procedure provides a method to determine the resistance of polypropylene to


embrittlement by high temperature (oxidation) exposure. This test provides insight on long
term thermal stability of a polypropylene battery container and cover.

4.1.2.2. Apparatus

4.1.2.2.1. Forced draft oven, capable of maintaining prescribed temperature within ±3ºC. The oven
must be designed to allow substantial unobstructed circulation of air around test specimens
placed in the oven.

4.1.2.2.2. Temperature measuring device – thermometer, copper constantan (Type T) thermocouple


and potentiometer, or other suitable device capable of measuring the temperature to ±3ºC.

4.1.2.2.3. Micrometer or other device suitable for measuring the test specimen thickness to the nearest
.02 mm or .001 in.

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4.1.2.2.4. Miscellaneous cutting tools for preparation of the test specimen.

4.1.2.3. Procedure

4.1.2.3.1. The test specimen to be used is to be a 1.524 mm ± 0.050 mm (0.060 in ± 0.002 in) thick
molded plaque cut approximately 38.1 mm (1.5”) in length by 50.8 mm (2”) in width. The test
specimen must be free of air inclusions and foreign materials (injection molded preferred).
Samples must also be free of rough edges for “fuzz” generated during the process of cutting
the test specimen.

4.1.2.3.2. All test specimens are to be coded for identification purpose.

4.1.2.3.3. Record the following information concerning each test specimen:

(a) Polymer type, color, vendor and lot number.


(b) Location of test specimen in the oven.
(c) Oven temperature
(d) Date that the test specimen was placed into the oven.

4.1.2.3.4. Suspend the test specimens in a clean oven in a suitable arrangement to allow at least a ½
inch space between each test specimen. There shall be no contact between the test
specimens or between the test specimen and the metal surface of the oven.

4.1.2.3.5. The test shall be conducted at a temperature of 149ºC ± 3ºC (300º ± 5ºF)

4.1.2.3.6. Test specimen to be visually inspected every twenty-four (24) hours for evidence of the
following:

(a) Embrittlement (cracking or crumbling of the test specimen). Note: This phenomenon
usually occurs first at the thinnest cross-section of the test specimen and is the most common
type of failure mode.

(b) Melting of the test specimen.

(c) A pronounced color change of the test specimen by a comparison to a sample from the
original plaque retained in darkness at room temperatures. (The date and degree of such an
occurrence should be noted; however the test should not be terminated).

4.1.2.3.7. Criterion for termination of the test shall be the occurrence of embrittlement and/or melting of
the test specimen.

4.1.2.3.8. Compute the total days that each test specimen was maintained at the test temperature
before the failure occurred. Record this total as the final test result.

4.1.2.3.9. The report of test results shall include the following:

(a) Polymer type, color, vendor and lot number.


(b) Oven temperature maintained during test.
(c) Date that the test specimen was placed into the oven.
(d) The failure mode (embrittlement and/or melting).
(e) Total days to failure of the test specimen.

4.2. Plastic Containers

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4.2.1. Acid Resistance Tests

4.2.1.1. Scope

The following tests shall be performed on container samples to determine their resistance to
sulfuric acid solutions:

(a) Acid Absorption Test.


(b) Material Deterioration Test.
(c) Dimensional Change Test.

4.2.1.2. Apparatus

4.2.1.2.1. Reagent grade sulfuric acid – 1.300 ± .005 sp. gr. 80/80.

4.2.1.2.2. Cutting tools.

4.2.1.2.3. Mild detergent.

4.2.1.2.4. Weighing scale (accuracy to 0.001 g.).

4.2.1.2.5. Caliper or Micrometer, accurate to 0.02 mm (0.001 in.).

4.2.1.2.6. Circulating air oven, temperature controllable at 65ºC ± 1ºC (150ºF ± 2ºF).

4.2.1.3. Procedure

4.2.1.3.1. Material samples shall be cut from flat areas and have four (4) cut sides.

4.2.1.3.2. Material samples shall not include gates, partition ribs, logos, nameplates or other
nonconformities.

4.2.1.3.3. Material samples shall consist of 26 sq. cm. (4 sq. in.) or as large as possible without
including the items mentioned in 4.2.1.3.2.

4.2.1.3.4. Material samples shall be cut to the specified dimensions. (Ref. Figure B). The cut edges
shall be essentially perpendicular to the flat surface of the sample, free of saw marks, nicks,
grooves or ragged edges.

Care shall be taken to insure that the flat surfaces of the samples are not scratched or
damaged and that the samples are not overheated or mechanically damaged during
preparation of the sample.

4.2.1.3.5. Samples shall be washed clean with a mild detergent and water solution and then rinsed with
water and air dried for at least 24 hours before pretest measurements are taken.

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Figure B

4.2.1.3.6. Measure to the nearest 0.02 mm (0.001 Inch) and record the length and width of the plane
surface of the sample at all locations as shown in Figure B.

4.2.1.3.7. Measure to the nearest 0.02 mm (0.001 inch) and record the thickness of the sample at the
four (4) locations as shown in Figure B.

4.2.1.3.8. Measurements specified in 4.2.1.3.6-7 shall be recorded and identified as shown in Figure B.

4.2.1.3.9. Weigh the sample and record the weight to the nearest milligram (0.001 g).

4.2.1.3.10. Samples should not exhibit the following conditions before testing: cracks, blisters, pitting,
swelling or discoloration.

4.2.1.3.11. All of the tests specified within the SCOPE shall be performed concurrently on the same
sample.

4.2.1.3.12. Completely immerse the weighed and measured sample in a glass container filled with the
sulfuric acid solution. The sample must be held beneath the surface of the liquid.

4.2.1.3.13. Cover the container tightly to prevent evaporation.

4.2.1.3.14. Place the container with the sample in a circulating-air oven with the temperature controlled
at 65ºC ± 1ºC (150ºF ± 2ºF) for 28 days.

4.2.1.3.15. Remove the container with the sample after 28 days and allow to cool to room temperature.

4.2.1.3.16. Remove the sample and rinse in running tap water to wash off the sulfuric acid solution and
dry the surface of the sample.

4.2.1.3.17. Examine the sample and record evidence of material deterioration with respect to the
conditions specified in paragraph 4.2.1.3.10 or other signs of material deterioration.

4.2.1.3.18. Weigh the sample in accordance with paragraph 4.2.1.3.9.

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4.2.1.3.19. Measure the width, length and the thickness of the sample in accordance with paragraph
4.2.1.3.6-7.

4.2.1.3.20. Calculate the dimension change percentage in each of the length, width and thickness
dimensions as follows:

Dimension Change Percentage + 100((MA – MB)/MB, Where MB = dimension of sample


before the test and MA = dimension of sample after the test.

4.2.1.3.21. Calculate the change of weight percentage as follows:

Change of Weight Percentage = 100((WA-WB)/WB), where WB = weight of sample before


the test in milligrams and WA = weight of sample after the test in milligrams.

4.2.1.3.22. The test report should include the following:

Name of manufacturer.

Manufacturing information (if available) such as size, date of manufacture, material, etc.

Date and time sample was placed in and removed from the oven.

The average, reported to the nearest 0.1 percent, of the two length dimension change
percentages calculated in paragraph 4.2.1.3.20.

The average, reported to the nearest 0.1 percent, of the two width dimension change
percentages calculated in paragraph 4.2.1.320.

The average, reported in the nearest 0.1 percent, of the four thickness dimension change
percentages calculated in 4.2.1.3.20.

Change of weight percentage calculated in paragraph 4.2.1.3.21, reported to the nearest 0.1
percent.

Evaluation of the condition of the sample before and after the test with respect to each of the
conditions of paragraph 4.2.1.3.10.

4.2.2. Impact Resistance

4.2.2.1. Scope

This procedure provides a method to determine the amount of force required to rupture a
battery container.

4.2.2.2. Apparatus

4.2.2.2.1. An impact missile with a contact radius of 30 mm (1.183 in.). This is the equivalent of a 0.91
kg (2 lb.) steel ball.

4.2.2.2.2. Cold box capable of maintaining -18ºC (0ºF).

4.2.2.2.3. Measuring device, 0-100 cm. or 0-36 in.

4.2.2.3. Procedure

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4.2.2.3.1. To be free fall tested on a container at –18ºC ± 1ºC (0ºF ± 2ºF). This procedure can be used
at other temperatures providing the temperature used is recorded on the report.

4.2.2.3.2. The container to be tested shall be conditioned at the test temperature for a minimum of eight
(8) hours.

4.2.2.3.3. Calculation of average impact values shall be made separately for end and side walls.

4.2.2.3.4. Alternate cells shall be tested, i.e., 1/3/5 on front and 2/4/6 on rear, with the proviso that no
cell shall have more than one (1) impact drop conducted on it. The front and back walls of
end cells will not be tested if end walls are to be tested on a single container, due to possible
adverse effect on end wall impact values. Impact values may be influenced by the container
geometry, i.e. on end cells near corners and on structural or cosmetic features on the
container.

4.2.2.3.5. Point of impact shall be at the intersection of L/2 and H/3 (or vary to H/2 from the bottom if
surface variation prevents testing at H/3) as shown in Figure C.

Figure C: Impact Point for Plastic Containers

4.2.2.3.6. The “Bruceton” method of conducting the impact testing is recommended. This procedure is
listed as “The Up-And-Down Design” (10-4) in the National Bureau of Standards Handbook
91.

4.2.2.3.7. Report the impact required to produce the first surface rupture of the container material.
Surface failure may be verified by electrical breakdown test, leak test, or other appropriate
method.

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4.2.2.3.8. Impact values may be influenced by the container geometry, i.e. on end cells near corners
and on structural or cosmetic features on the container.

4.2.3. Bulge Test

4.2.3.1. Scope

This procedure provides a method for determining the end wall bulge characteristics of a
battery container.

4.2.3.2. Apparatus

4.2.3.2.1. Metal tray.

4.2.3.2.2. Commercial grade polyethylene glycol

4.2.3.2.3. Oven capable of maintaining 93ºC (200ºF).

4.2.3.2.4. Measuring instrument accurate to 0.02 mm (0.001 in.).

4.2.3.3. Procedure

4.2.3.3.1. Place an empty container with flat end walls in an appropriate rigid metal tray. Concave or
convex end walls may effect test results.

4.2.3.3.2. Fill the container to within 25 mm (1 inch) of the top with commercial grade polyethylene
glycol at a temperature of 93ºC ± 3ºC (200ºF ± 5ºF).

4.2.3.3.3. Place the tray containing the container to be tested in an oven and maintain the polyethylene
glycol at 93ºC ± 3ºC (200ºF ± 5ºF).

4.2.3.3.4. When the liquid in the end cell adjacent to the end wall to be measured reaches a
temperature of 93ºC ± 3ºC (200ºF ± 5ºF), start a one hour soak time.

4.2.3.3.5. At the end of the soak period, remove the tray containing the container being tested from the
oven and within five minutes measure the end wall bulge. The polyethylene glycol is to
remain in the test container until the completion of the measurements.

4.2.3.3.6. The bulge shall be determined by comparing the center of the end wall with the plane of the
four corners exposed. The center of the end wall is defined as a point half way between the
horizontal parting line at the bottom and the bottom of the top band.

4.2.3.3.7. Bulge is to be reported as the difference as determined in (4.2.3.3.6).

Bulge values may be influenced by the container geometry, i.e. structural or cosmetic
features. Bulge values may not be representative of a finished battery (a sealed cover would
fixture the top of the end wall).

4.2.4. Electrical Breakdown

4.2.4.1. Scope

The purpose of this test is to qualify containers for use in lead acid battery applications.

4.2.4.2. Apparatus

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4.2.4.2.1. Conductors – close fitting mandrel or suitable liquid equivalent

4.2.4.2.2. Transformer capable of maintaining 30,000 volts.

4.2.4.3. Procedure

4.2.4.3.1. Safety precautions should be taken to avoid electrical shock.

4.2.4.3.2. The container shall be fitted with a close fitting mandrel and outer shield to within 38 mm (1.5
in.) of the top, or a suitable liquid equivalent.

4.2.4.3.3. A minimum potential of 15,000 volts, or 100 volts per mil thickness (as specified on the
container design drawing), whichever is greater, but not to exceed 30,000 volts maximum,
shall be applied to the test area of the container for not more than five seconds.

4.2.4.3.4. Inspect the container for evidence of being perforated or burned through.

4.2.5. Adhesion

4.2.5.1. Scope

This procedure provides a method for determining the adequacy of flame treatment by
observing how well a specific ink solution adheres to the treated surface.

4.2.5.2. Apparatus

Felt-tipped marking pens designed for checking surface tension of treated polymers. Dyne
rate of 38 – 40 minimum.

(a) Corotec Corporation


P.O. Box 386
Collinsville, CT 06022

Poly Test Pen


38 Dyne level

(b) Independent Ink


14705 S. Avalon Blvd.
Gardena, CA 90248

Poly Treat Check Pen


38-40 Dyne level

4.2.5.3. Procedure

4.2.5.3.1. The test must be performed in a clean and dry environment. Extreme moisture, even very
high humidity, has a deleterious effect on the test. Never try to make a test near an open
door, during, or soon after a rain.

4.2.5.3.2. Using the broad tip of the marker, lightly apply a single line on all bonding surfaces. Interpret
results based on manufacturer’s recommendations.

4.2.5.3.3. This test follows closely the procedure outlined in ASTM method D 2578-84. Refer to the
ASTM method when questions arise.

4.2.6. Tensile Pull Test for Side Terminals

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4.2.6.1. Scope

This procedure provides a method to determine the tensile strength of a side terminal.

4.2.6.2. Apparatus

Figure D: Test Fixture 1

4.2.6.2.1. Steel rod. One end is to be machined square to fit into the tester grips and the opposite end
is to be threaded to fit into the nut of the terminal. Figure D.

4.2.6.2.2. Fixture, with hole in center to run the steel rod through, to restrain the face of the terminal
from undue movement during test. Figure D.

4.2.6.2.3. Tinius Olsen LoCap Tester, or equivalent.

4.2.6.2.4. Shim stock of sufficient thickness and diameter to place under the terminal boss not being
tested, to support it over the upper crosshead.

4.2.6.3. Procedure

4.2.6.3.1. Age the side terminal sample(s) at an ambient room temperature of 24ºC – 27ºC (75ºF –
80ºF) for a minimum of eight hours before testing.

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4.2.6.3.2. Adjust load dial to zero. Tester speed: 12.5 mm/minute (0.5”/minute).

4.2.6.3.3. Place the fixture to restrain the face of the terminal to be tested over the top of the hole in the
upper crosshead.

4.2.6.3.4. Place the terminal or the container to be tested over the restraining fixture.

4.2.6.3.5. Apply the tensile load continuously at a jaw separation rate of 12.5 mm/minute (0.5”/minute).

4.2.6.3.6. The failure point will be interpreted as occurring when the tensile value stops increasing.
Report this value in kilograms (pounds) of load for the terminal tested.

4.2.7. Torque Test for Side Terminals

4.2.7.1. Scope

This test measures the torque resistance between the nut and lead terminal assembly and
the container material and the lead assembly.

4.2.7.2. Apparatus

4.2.7.2.1. Torque wrench. P.A. Sturtevant, Div of Dresser Industries Model 1S, 0-35 Joules or or 0-300
inch-pounds capacity or equivalent.

4.2.7.2.2. Appropriate holding fixture.

4.2.7.2.3. Reference: Figure E: Test Fixture 2.

Figure E

4.2.7.2.4. 7.9 mm (5/16 in) size socket.

4.2.7.3. Procedure

4.2.7.3.1. Age the side terminal container sample(s) to an ambient room temperature of 24ºC – 27ºC
(75ºF – 80ºF) for a minimum of eight hours before testing.

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4.2.7.3.2. Place and secure the side terminal container in appropriate holding fixture to prevent
movement during test.

4.2.7.3.3. Connect the adapter to the terminal in the container and hand tighten the stud until snug.

4.2.7.3.4. With the torque wrench in place and set in the zero position and the container firmly secured,
begin applying the torque in a direction perpendicular to the axis of the side terminal and
parallel to the side of the container.

4.2.7.3.5. Report the maximum torque value, that is the point at which the original (first) loss of torque
occurs, as well as the reason for failure (Example: 28 Joules (250 inch-pound) lead rotating
inside the container material and/or nut pulling up inside the lead, etc.)

4.2.8. Leakage Test for Side Terminals

4.2.8.1. Scope

This procedure provides a method for determining if a leak exists at the side terminal of a
battery container.

4.2.8.2. Apparatus

4.2.8.2.1. Pressure tester capable of maintaining the preset pressure as defined in 4.2.8.3.4 of the test
procedure and testing in accordance with 4.2.8.3.5 of the test procedure.

4.2.8.2.2. A cell closure device designed to mate with the upper edges of the container and prevent
escape of air from inside the cell being tested.

4.2.8.2.3. Eye dropper

4.2.8.2.4. Leak test solution – mixture of liquid detergent and water.

4.2.8.3. Procedure

4.2.8.3.1. Age the container sample a minimum of eight hours at room temperature before testing

4.2.8.3.2. Place the closure device over the cell containing the terminal to be tested

4.2.8.3.3. Position the container with the closure device in place, on its side with the lead terminals
facing upwards.

4.2.8.3.4. Activate the cylinder control to position and seal the outer edges of the cover tongue against
the sponge rubber.

NOTE: Cylinder pressure should be preset at 2.5 kg/cm2 (35 psi.).

4.2.8.3.5. The pressure gauge for regulating the air pressure to the container should be preset at .35
kg/cm2 (5 psi.).

4.2.8.3.6. Using eye dropper, slowly add leak test solution to outer surface of insert, making sure the
junction of lead and molded container material is covered. Also put solution inside the
threaded hole of the insert. The solution on the test surfaces shall be free of bubbles.

4.2.8.3.7. With the container under pressure, in this position for two (2) minutes, observe the test
solution for signs of leakage indicated by bubbles. Report bubbles per minute.

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4.3. Plastic Covers

4.3.1. Acid Resistance

Follow the test procedure use for containers. Reference 4.2.1

4.3.2. Impact Resistance

4.3.2.1. Scope

This procedure provides a method to determine the amount of force required to rupture a
battery cover.

4.3.2.2. Apparatus

4.3.2.2.1. An impact missile with a contact radius of 30 mm (1.183 in.). This is the equivalent of a 0.91
kg (2 lb.) steel ball.

4.3.2.2.2. Cold box (capable of maintaining -18ºC (0ºF))

4.3.2.2.3. Measuring device, 0-100 cm or 0-36 in.

4.3.2.3. Procedure

4.3.2.3.1. To be free fall tested on a container at –18ºC ± 1ºC (0ºF ± 2ºF). This procedure can be used
at other temperatures providing the temperature used is recorded on the report.

4.3.2.3.2. The cover to be tested shall be conditioned at the test temperature for a minimum of eight
hours.

4.3.2.3.3. Seat the cover on an appropriate container, or equivalent, in such a manner that the sealing
surfaces of the cover are rigidly supported. The test should be done on intermediate and
terminal cells.

4.3.2.3.4. Standard single wall covers:

(a) Impact on a flat surface as near the center of the cell as possible.

(b) The impact point should not be over a partition, rib or reinforced area.

4.3.2.3.5. Two piece/double wall covers, sealed manifold vent systems, with and without removable
plugs.

(a) Impact test the covers after the finished cover or manifold covers have been sealed in
place.

(b) Impact on the flat surface of both single and double walled areas, as near the center of
the unsupported section as possible.

(c) The impact point should not be over a partition, rib or reinforced area.

4.3.2.3.6. The “Bruceton” method of conducting the impact testing is recommended. This procedure is
listed as “The Up-And-Down Design” in the National Bureau of Standards Handbook 91.

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4.3.2.3.7. Report the impact required to produce the first surface rupture of the cover material. Surface
failure may be verified by electrical breakdown test, leak test, or other appropriate method.

4.3.3. Bushing Impact Resistance

4.3.3.1. Scope

This procedure provides a method to determine the amount of force required to rupture a
battery cover when impacted directly on the terminal bushing.

4.3.3.2. Apparatus

4.3.3.2.1. An impact missile with a contact radius of 30 mm (1.183 in.). This is the equivalent of a 0.91
kg (2 lb.) steel ball.

4.3.3.2.2. Cold box capable of maintaining –18ºC (0ºF).

4.3.3.2.3. Measuring device, 0-100 cm or 0-36 in.

4.3.3.2.4. Flanged brass pin.

4.3.3.3. Procedure

4.3.3.3.1. To be free fall tested on a container at –18ºC ± 1ºC (0ºF ± 2ºF). This procedure can be used
at other temperatures providing the temperature used is recorded on the report.

4.3.3.3.2. The cover to be tested shall be conditioned at the test temperature for minimum of eight
hours.

4.3.3.3.3. Seat the cover on an appropriate container, or equivalent, in such a manner that the sealing
surfaces of the cover are rigidly supported.

4.3.3.3.4. Insert the brass pin into the inside of the lead bushing. Seat the flange on the top surface of
the bushing. The test should be done on both positive and negative terminals.

4.3.3.3.5. The impact missile shall hit in the center of the flanged pin.

4.3.3.3.6. The “Bruceton” method of conducting the impact testing is recommended. This procedure is
listed as “The Up-And-Down Design” (10-4) in the National Bureau of Standards Handbook
91.

4.3.3.3.7. Report the impact required to produce the first surface rupture of the cover material. Surface
failure may be verified by electrical breakdown test, leak test, or other appropriate method.

4.3.4. Bushing/Stud Torque Test

4.3.4.1. Scope

This procedure provides a method for measuring the torque resistance between the stud and
lead terminal assembly, and the cover material and the lead bushing assembly.

4.3.4.2. Apparatus

4.3.4.2.1. Torque wrench, P.A. Sturtevant, Div. of Dresser Industries, Model M300-1S, 3/8 inch square
drive size, 0-35 joules or 0-300 inch-pounds capacity, or equivalent.

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4.3.4.2.2. One set of positive and negative high profile lead bushing adapters (custom design) or a
ratchet drive stud extractor Snap-On A-36USA8 or equivalent.

4.3.4.2.3. Pins sized to fit the inside of the bushings.

4.3.4.2.4. Fixture to hold cover in place.

4.3.4.2.5. Acorn nut (used for stud testing).

4.3.4.3. Procedure

4.3.4.3.1. Obtain the cover sample to be tested from any point after flame treating.

4.3.4.3.2. Age the flame treated cover sample to an ambient room temperature of 24ºC - 27ºC (75ºF -
80ºF) for a minimum of eight hours before testing.

4.3.4.3.3. Place pin into the correct high profile lead bushing, making sure that it is seated all the way
down. Install bushing adapters or stud extractor. Use an acorn nut when testing a stud type
terminal.

4.3.4.3.4. With the torque wrench in the zero position and the assembly firmly secured, begin applying
the torque in a direction perpendicular to the axis of the high profile lead bushing and parallel
to the top of the assembly.

4.3.4.3.5. Report the maximum torque value at the point of failure as well as the reason for failure. For
example: bushing rotating inside of plastic as opposed to cohesive lead failure, etc.

NOTE: For covers with low profile bushings, using samples obtained after flame treatment (if
applicable), form the necessary SAE terminal posts on the cover and then proceed to test as
outlined in above procedure.

4.3.5. Adhesion

Follow the test procedure used for containers. Reference 4.2.5.

5. SEPARATOR TEST METHODS

5.1. Test I – Ohmic Resistance

5.1.1. Procedure IA – Pre-Treatment

5.1.1.1. Scope

This method covers the conditioning of separator samples prior to the resistance
measurement.

5.1.1.2. Applicable Documents

Procedure 1B Ohmic Resistance (Paragraph 5.1.2)

5.1.1.3. Significance and Use:


The measured resistance of a sample varies with the degree of saturation. The time required
for saturating the sample with acid varies with temperature, acid strength, separator material
and pore size distribution. Standard practice in the industry is to measure ohmic resistance

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after soaking the samples for 20 minutes or 24 hours. In addition, separators with average
pore diameters of 1 micron or less are boiled before the ohmic resistance measurement. The
20 minute soak is used to simulate the resistance of the separator before formation. The 24
hour soak is used to simulate the resistance of the separator after formation. The boiled “E-R”
is the lowest reading one can obtain and approximates the resistance of the separator after
extended service.

5.1.1.4. Apparatus:

5.1.1.4.1. Container that is large enough to hold the ohmic resistance samples.

5.1.1.4.2. Sulfuric acid

Specific gravity – 1.280 (when corrected to 80ºF 26.7°C))

Temperature – 80ºF (26.7°C)

Purity – Battery grade is the minimum acceptable purity.

5.1.1.5. Procedure:

5.1.1.5.1. Cut sample to appropriate size (if necessary).

5.1.1.5.2. Soak sample(s) for 20 minutes or 24 hours in sulfuric acid.

5.1.1.6. Boiling Procedure for Materials With an Average Pore Diameter of One Micron or Less as
Measured by Mercury Intrusion

5.1.1.6.1. Apparatus:

(a) Container that is large enough to hold the ohmic resistance samples.

(b) Boiling distilled water.

5.1.1.6.2. Procedure:

(a) Cut sample to appropriate size (if necessary)

(b) Boil sample in distilled water for 10 minutes

(c) Remove sample from water and blot the sample dry, removing excess liquid.

(d) Soak the sample(s) in sulfuric acid for 20 minutes.

5.1.2. Procedure 1B – Ohmic Resistance

5.1.2.1. Scope:

This method covers the test conditions, apparatus and procedure for the measurement of the
ohmic resistance of battery separators.

5.1.2.2. Applicable Documents:

Procedure 1A Pre-treatment (Paragraph 5.1.1)

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5.1.2.3. Significance and Use:

The measured resistance of battery separators is used as a design tool and as a receiving
inspection parameter by battery companies. It is also used as an internal quality control
parameter by the separator industry.

5.1.2.4. Definition:

The ohmic resistance of battery separators is defined as the increase in electrolyte resistance
caused by the pore structure of the separator.

5.1.2.5. Apparatus:

5.1.2.5.1. Digital AC ohmmeter or impedance bridge with sufficient resolution to indicate a 1% change
in the measured resistance.

5.1.2.5.2. Resistance measuring cell that uses a fixed area of the sample for the measurement.

5.1.2.5.3. Sulfuric Acid

Specific gravity – 1.280 ± .005 (corrected to 80ºF (26.7°C))

Temperature – 80ºF 26.7°C)

Purity – Battery grade is minimum acceptable purity. For critical measurements and where
readings form different locations are being compared, use fresh reagent grade sulfuric acid.

5.1.2.5.4. The Palico Low Resistance Measuring System is used as the example for this type of
apparatus. A drawing of the cell is included in this procedure.

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5.1.2.6. Test Specimens

Cut samples such that they are larger than the fixed area window and can be pulled out of
the cell by hand.

Most automotive battery separators will fit into the Palico cell without cutting.

5.1.2.7. Preparation of the Apparatus

5.1.2.7.1. Make certain that the electronics are stabilized. If the meter includes a setting that uses a
standard resistance (“Standby” on the Palico), the meter reading should be within 1% of the
value of the resistor.

5.1.2.7.2. For the Palico 9100-2 system, BCI standard configuration is:

Voltage Electrode Shunt – 1100 Ohms

Current Electrode Shunt – 4700 Ohms

Aperture Size – Circular with total area of 5 square inches

Number of Samples – Measure 1 sample at a time

5.1.2.8. Procedure

5.1.2.8.1. Follow the appropriate pretreatment procedure and put the samples into the storage
compartment of the cell in the following manner:

Support the samples at a 30 degree angle from the horizontal such that only the first half inch
of sample is immersed in the acid.

Allow the acid to wick into the sample. As wicking continues, immerse the wet area of the
separator. This method of sample insertion allows air to escape from the pores of the
separator and is especially important in routine 20 minute “E.R.” measurements.

5.1.2.8.2. Apply current to the cell. Check for D.C. polarization on the voltage electrodes. If more than
100 mV (0.1V) is present, allow 30 minutes for stabilization and/or discharge of the
polarization. If polarization persists, the acid must be changed and the electrodes cleaned.

5.1.2.8.3. Check the resistance of the cell. Agitate the acid to make certain that the cell resistance is
constant. On the Palico cell, move the gate back and forth a few times. The cell resistance
should be fairly constant at a given temperature, acid concentration, and barrier resistance,
varying less than 5%.

5.1.2.8.4. If all of the above conditions are met, insert the first separator in the test area and close the
gate. Do not close the gate so tightly that the separator cannot be pulled out by hand. The
sample must be removed by hand in Step 5.1.2.8.6

5.1.2.8.5. Read the cell resistance including the separator. If the digital display drifts, wait until it
fluctuates over the same range. Use the lowest range that you can to achieve the best
resolution, then record the mean value as the reading. This is RT in the calculation.

5.1.2.8.6. Remove the separator from the test area with one hand. Do not move the gate.

5.1.2.8.7. When the display fluctuates over the same range record the mean value. This is RC in the
calculation.

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5.1.2.8.8. Repeat this procedure for the number of samples to be tested.

5.1.2.8.9. Insert a sheet of solid plastic or glass that has the same dimensions (height and width) as the
separator sample.

5.1.2.8.10. Close the gate such that the plastic sheet can be removed with one hand.

5.1.2.8.11. Adjust the range of the meter to obtain a reading. Record this reading when it is stable. (It will
rise for a while after the gate is closed.). This is RB in the calculation.

5.1.2.9. Calculations:

5.1.2.9.1. RS = RT – RC

RC is the value obtained in Step 5.1.2.8.7


RT is the value obtained in Step 5.1.2.8.5
RS is the resistance of the measured separator area.

5.1.2.9.2. “E-R” = RS x Aperture Area

“E-R” is the resistance of one unit area of the separator.

5.1.2.9.3. Correct the “E-R” for barrier resistance and overall thickness:

“E-R” (corrected) = “E-R” x (1 + (.008 x OA x RC/RB)).


RB is the value obtained in Step 5.1.2.8.11
OA = overall thickness in mils (thousandths of 1 inch).

5.1.2.9.4. Use either ohms or milliohms for all values. Do not mix values.

5.1.2.10. Maintenance of Equipment:

5.1.2.10.1. If the ration of RC/RB is less than .015, the barrier resistance correction is unnecessary.
Even at an overall thickness of 100 mils, the correction factor is less than 1.5%. In the Palico
cell, one way to achieve this condition is to seal the voltage electrode partitions to the walls
and floor of the cell. A cell with sealed partitions is harder to clean but is more stable
electrically and mechanically.

5.1.2.10.2. If the barrier resistance (RB) and the cell resistance (RC) are stable, one can establish the
corrections as a set of curves for various separator types and avoid doing this calculation
whenever measurements are made. However, the barrier resistance and cell resistance
should be measured whenever the acid is changed or if the cell is moved. They should also
be checked periodically because the cell is usually made of plastic. Plastic warps with time
and this would cause changes in the resistance readings.

5.1.2.10.3. If the bath must be dried for shipment, storage or any other reason, pour the acid out and re-
fill the bath with water. Allow it to stand for 24 hours. Then drain it and allow it to dry at room
temperature.

5.1.2.10.4. Correct the readings for temperature by multiplying the “E-R” value by the correction factor.

Temperature °F (°C) Correction Factor


84 (28.9) 1.04
83 (28.3) 1.03
82 (27.8) 1.02

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81 (27.2) 1.01
80 (26.7) 1.00
79 (26.1) 0.99
78 (25.6) 0.98
77 (25.0) 0.97
76 (24.4) 0.96

These factors are calculated from sulfuric acid conductivity data in Lead Acid Batteries by
Hans Bode (Wiley, New York, 1977, pp. 73-77).

5.1.2.11. Procedure for BCI Cells with Analog Potentiometers

5.1.2.11.1. Apparatus:

(a) Analog potentiometer with sufficient resolution to indicate a 1% change in the measured
resistance.

(b) Resistance measuring cell.

(c) Sulfuric acid:


Specific gravity – 1.280 ± .005 (corrected to 80ºF/80°F (26.7°C/26.7°C)).
Temperature – 80ºF (26.7°C).
Purity – battery grade is minimum acceptable purity. For critical measurements and where
readings from different locations are being compared, use fresh reagent grade sulfuric acid.

(d) The BCI (formerly AABM) cell with Leeds and Northrup Kelvin Bridge is used as a specific
example for this type of apparatus. A drawing of the cell is included in this procedure

(e) For the BCI system, the standard sample size is 4-13/16 x 4-13/16 inches 122 mm x 122
mm) square. The cell measures the resistance of a group of 5 separators in series.

- The following is BCI standard apparatus (See Drawing No. AC-3727):

- A.C. Kelvin Bridge Ohmmeter, Leeds & Northrup Cat. No. 4286, or equivalent.

- Separator resistance testing tank, Drawing No. AC-3725.

- Graphite electrodes, Dixon’s H80-D graphite plates from Joseph Dixon Crucible Co., Wayne
and Monmouth Streets, Jersey City 3, New Jersey, or equivalent, cast in lead bars as per
Drawing No. 3726.

- Four rubber-covered, single conductor, #14 cables with lugs and special fittings to connect
to Kelvin Bridge terminal posts.

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(f) Water bath, or other suitable device, to maintain temperature of testing tank.

(g) Paper cutter for cutting separators to standard dimensions.

5.1.2.11.2. Test Specimens:

The size and number of test specimens is as given in the manufacturer’s instructions.

5.1.2.11.3. Preparation of Equipment:

Adjust the Kelvin Bridge as follows:

(a) Connect the potential and current leads form the electrodes to the corresponding
terminals on the Kelvin Bridge as shown in Drawing No. AC-3727.

(b) Connect bridge to AC power source and allow instrument to warm up at least 30 minutes
before starting test.

(c) Place resistance plug in the position marked “1”.

(d) Release the galvanometer needle and move the zero adjustment until the needle rests on
zero.

(e) Hold down the button marked “A.C.” and turn the slide wire knob in the same direction
that the galvanometer needle is off zero to bring needle back to the zero position.

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(f) Release “A.C.” button and check to see if needle rests on zero. Repeat Steps 5.4 and 5.5
until needle does not move when the “A.C.” button is either up or down.

(g) The bridge is now in balance and is ready for the tests.

5.1.2.11.4. Procedure:

(a) Follow the appropriate pretreatment procedure and put the samples into the storage
compartment of the cell in the following manner:

Support the samples at a 30 degree angle from the horizontal such that only the first half inch
of sample is immersed in the acid.

Allow the acid to wick into the sample. As wicking continues, immerse the wet area of the
separator. This method of sample insertions allows air to escape form the pores of the
separator and is especially important in routine 20 minute “E-R” measurements.

(b) Acid level – Adjust acid level such that the separators are just covered with acid when in
the test area.

(c) Select 5 separators at random for the test.

(d) Measure the cell resistance, with the separators in the end compartment of the testing
tank, by holding down the “A.C.” button and turning the slide wire in the direction that the
galvanometer needle is off zero until the bridge is again balanced. Record this value directly
from the dial. This is RC in the calculation.

(e) Place the separators in the test area between the potential electrodes with the separator
ribs running vertically. The level of the electrolyte shall be exactly that of the top of the
separators. Be sure air has been removed from separators.

(f) Measure the resistance when the separators are in the central compartment of the testing
tank again holding down the “A.C.” button and turning the slide wire in the direction that the
galvanometer needle is off zero until the bridge is again balanced. Record this value directly
from the dial. This is RT in the calculation.

(g) Repeat this procedure for the number of samples that you have.

(h) Place a sheet of solid plastic in the test area that is cut to the same height and width as
the separators.

(i) Press the “A.C.” button and balance the bridge. If you cannot balance the bridge, release
the “A.C.” button and move the range plug to the position marked “10”.

(j) Balance the bridge. Multiply the reading by 10 and record. This is RB in the calculation.

This barrier resistance measurement should be done with each group of separators. Test
area is partially dependent on liquid level in this cell. Therefore, one can expect the barrier
resistance to vary from day to day.

5.1.2.11.5. Calculations

(a) RS = (RT – RC)/5


RC is the value obtained from 5.1.2.11.4(d).
RT is the value obtained from 5.1.2.11.4(f).

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RS is the resistance of one separator.

(b) “E-R” = RS x separator area


For 4-13/16” square samples: “E-R” = RS x 23.2.
“E-R” is the resistance of one unit area of the separator.

(c) Correct the “E-R” for barrier resistance and overall thickness:
“E-R” (corrected) = “E-R” x (1 + (.008 x OA x RC/RB)).
RB is the value obtained from 5.1.2.11.4(j).
OA = overall thickness in mils (thousandths of one inch).

(d)Use either ohms or milliohms. Do not mix units.

(e) Correct the readings for temperature by multiplying the “E-R” value by the correction
factor.

Temperature ºF (°C) Correction Factor


84 (28.9) 1.04
83 (28.3) 1.03
82 (27.8) 1.02
81 (27.2) 1.01
80 (26.7) 1.00
79 (26.1) 0.99
78 (25.6) 0.98
77 (25.0) 0.97
76 (24.4) 0.96

These factors are calculated from sulfuric acid conductivity data in Lead Acid Batteries by
Hans Bode (Wiley, New York, 1977, pp. 73-77).

5.1.2.11.6. Maintenance of Equipment:

(a) When casting the graphite plates in lead bars it is important to heat the mold for the lead
bar to a temperature close to that of the molten lead to obtain a casting with intimate contact
between graphite and lead.

(b) There should be no difficulty in balancing the Kelvin Bridge, but should there be any
trouble, the cause must be determined and corrected before making ohmic resistance
measurements. Corrosion and poor contact in the leads connecting the bridge and the
electrodes are the most probable cause of trouble.

(c) Care should be taken to see that the separators are completely submerged in the
electrolyte during soaking.

(d) The fringe of acid around the sides and over the top of the separators must be carefully
eliminated or controlled. If the separators are cut to the proper width and height, and the acid
level is correct, any fringe resistance is consistent. When the acid level is allowed to come ¼
inch above the separators, or the separators are cut ¼ inch too narrow, the decrease in
separator resistance will be 10% or more. Some separators have enough buoyancy to float
off the bottom of the tank unless care is taken to keep them in position. Any error that might
be caused by a fringe of acid on the bottom of the separators may be eliminated by holding
the nest of separators against the bottom of the tank, usually accomplished by laying a glass
stirring rod, or other suitable non-conductor, on the separators.

(e) If the bridge cannot be balanced with the resistance plug in the position marked “1”, place
the plug in the position marked “10” and multiply the resistance reading by this amount.

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(f) If the ratio of RC/RB is less than .015, the barrier resistance correction is unnecessary.

(g) If the barrier resistance (RB) and the cell resistance (RC) are stable, one can establish the
corrections as a set of curves for various separator types and avoid doing this calculation
whenever measurements are made. However, the barrier resistance and cell resistance
should be measured whenever the acid is changed or if the cell is moved. They should also
be checked periodically because the cell is usually made of plastic. Plastic warps with time
and this would cause changes n the resistance readings.

5.2. Test II – Dimension Measurement

5.2.1. Procedure IIA – Height and Width

5.2.1.1. Scope: This procedure covers two methods of measuring height (length) and width of battery
separators.

5.2.1.2. Significance and Use:

5.2.1.2.1. Method A is applicable to separators up to 24 inches or 0.6 meter in height for automotive or
traction type separators.

5.2.1.2.2. Method B is applicable to large separators for industrial type batteries.

5.2.1.3. Definition:

5.2.1.3.1. HEIGHT is the dimension of the edge that is parallel to a vertical rib. It is also called length.

5.2.1.3.2. WIDTH is the dimension of the edge that is perpendicular to a vertical rib.

5.2.1.4. Method A

5.2.1.4.1. Apparatus:

(a) Carpenter square graduated in 1/32 inch (0.0313 inch or 0.5 mm increments and equal to
or greater in length than the largest separator to be measured.

(b) The square is mounted in a flat smooth work surface.

(c) Certified gage blocks to calibrate dimensional accuracy.

5.2.1.4.2. Procedure:

(a) Sheet or Leaf Separator (Height and Width).

Place the separator into the corner of the square with rib side up. Be sure the separator is
pressed flat to the work surface and fully contacting both square rule edges along entire
height and width.

Read and record height and width dimensions to the nearest 1/32 inch or to the nearest 0.5
mm.

(b) Roll-form Separator for Enveloping (Width only).

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Cut a section of appropriate length for the measuring apparatus. Square one (or both) end(s)
and proceed to measure as described in Step 5.2.1.2.4(a) above.

5.2.1.5. Method B

5.2.1.5.1. Apparatus:

(a) Steel rule graduated in 1/32 inch or in 0.5 mm increments and equal to or greater in length
than largest separator to be measured.

(b) Flat smooth work surface.

(c) Certified gage blocks to calibrate dimensional accuracy.

5.2.1.5.2. Procedure:

(a) Place the rule against backside of separator.

(b) Measure the height by placing the rule at right angle with end of separator.

(c) Measure the width by placing the rule at right angle with sides of separator.

(d) Read and record height and width dimensions to the nearest 1/32 inch or to the nearest
0.5 mm.

5.2.2. Procedure IIB – Squareness

5.2.2.1. Scope: This procedure is intended to provide a method of measuring the squareness of
separators.

5.2.2.2. Apparatus:

5.2.2.2.1. Square rule or squareness set-up plate which consists of a flat surfaced plate with locating
bars positioned at right angle.

5.2.2.2.2. Steel rule graduated in 1/64 inch (0.0156 inch) or 0.5 mm increments.

5.2.2.3. Procedure:

5.2.2.3.1. Place the separator to be checked on working surface or squareness set-up plate with rib
side up.

5.2.2.3.2. Place the long side of separator against vertical locating bar or vertical blade of square rule.

5.2.2.3.3. Slide the separator to the lower horizontal section of square rule or locating bar by sliding the
separator gently until one edge of the separator makes contact with horizontal bar while
keeping length edge of separator against vertical locating bar or vertical blade of square rule.

5.2.2.3.4. Measure squareness of separator as distance between horizontal bar and a separator edge.
Record squareness to the nearest 1/32 inch or to the nearest 0.5 mm.

5.2.2.3.5. Repeat above procedure after rotating separator 180º.

5.2.3. Procedure IIC – Backweb Thickness

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5.2.3.1. Scope: This procedure covers two methods of measuring backweb thickness of battery
separators.

5.2.3.2. Significance and Use:

5.2.3.2.1. Method A is applicable to separators with backweb space between ribs wider than ½ inch.

5.2.3.2.2. Method B is applicable to separators with backweb space between ribs from 3/16 inch to ½
inch.

5.2.3.3. Definition: All pressures are defined per unit area of the penetrator of the micrometer.

5.2.3.4. Apparatus:

5.2.3.4.1. Dial micrometer graduated in .001” increments, B.C. Ames Model #262. Federal Model 6591-
B-68 or equivalent.

5.2.3.4.2. For Method A – 3/8 inch (.375 inch) diameter contact foot for rib spacing over ½ inch (0.500
inch), 8 oz. (0.5 lb) top weight, (11 oz. total weight), 6.2 psi.

5.2.3.4.3. For Method B – 3/16 inch (.1875 inch) diameter contact foot for backweb between ½ inch
(0.500 inch) and 3/16 inch (0.1875 inch), no top weight (3 oz. total weight), 6.8 psi.

5.2.3.4.4. Certified gage blocks to calibrate micrometer.

5.2.3.5. Preparation of Apparatus:

5.2.3.5.1. Before measuring separator samples, make certain that the base plate and penetrator are
clean and operating smoothly without binding.

5.2.3.5.2. Check dial micrometer accuracy using certified gage blocks. Make sure dial micrometer is
zeroed when top and bottom feet are in contact.

5.2.3.6. Procedure:

5.2.3.6.1. Raise the penetrator sample rib side up on the base plate.

5.2.3.6.2. Gently lower the penetrator between the ribs until it contacts the backweb area. Do not allow
the penetrator to free fall onto the backweb.

5.2.3.6.3. Read the backweb thickness of the separator sample in the center and each edge to the
nearest 0.001”. Average the readings and compare to specification and tolerance.

5.2.4. Procedure IID – Overall Thickness

5.2.4.1. Scope: This procedure covers three methods of measuring the overall thickness of battery
separators at three different pressures.

5.2.4.2. Significance and Use:

5.2.4.2.1. Method A is applicable to measurement of most types of separators.

5.2.4.2.2. Method B is intended for industrial or submarine type separators with heavy rib design.

5.2.4.2.3. Method C is intended for automotive type separator with corrugated or embossed rib design.

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5.2.4.3. Apparatus:

Method A Method B Method C


Basic Gauge Dial Micrometer Ames Dial Micrometer Dial Micrometer Federal
Model 262 or equivalent Amerace Drawing or Model #691-B-68 or
equivalent equivalent
Dial Graduation .001 inch or .01mm .001 inch or .01mm .001 inch or .01mm
Base Ames Model #16 or Amerace Drawing or Federal Model #691-B-
equivalent equivalent 68 or equivalent
Penetrator Contact 2 inch diameter 3” x 3” square 2 inch diameter
Foot
Top Loading Weight 1.0 pounds 9 pounds .5 pound
Plus Penetrator
Surface Contact 0.3 pounds/square inch 1.0 pounds/square inch 0.16 pounds/square
Pressure inch

5.2.4.4. Procedure:

5.2.4.4.1. Before measuring separator samples, make certain that the base plate and penetrator are
clean and operating smoothly without binding.

5.2.4.4.2. Check micrometer accuracy using certified gauge blocks. Be sure dial micrometer is zeroed
when top and bottom feet are in contact.

5.2.4.4.3. Raise the penetrator and insert separator sample rib side up on the base plate.

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5.2.4.4.4. Gently lower the penetrator down until it contacts the maximum number of ribs possible. Do
not allow penetrator to free fall on the separator.

5.2.4.4.5. Check overall thickness at each edge and in the center. Average the three readings and
compare to specification and tolerance. Read to the nearest 0.001 inch or to the nearest 0.01
mm.

5.3. Test III – Determination of Volume Porosity

5.3.1. Scope: This method is to measure the open pore volume relative to the total separator
volume.

5.3.2. Significance and Use:

5.3.2.1. The pore volume is relevant to both the electrical performance of the battery and the volume
of electrolyte displaced by the separators.

5.3.2.2. This method is not valid for separators made exclusively of materials that are less dense than
water.

5.3.3. Apparatus:

5.3.3.1. Balance, with an accuracy of 0.01g, fitted with a wire and hook.

5.3.3.2. 1 liter beaker.

5.3.3.3. Vacuum desiccator

5.3.3.4. Water aspirator or vacuum pump.

5.3.3.5. Paper cutter

5.3.3.6. Aerosol OT (Cyanamid) aqueous solution of 0.1% concentration.

5.3.4. Test Specimens:

5.3.4.1. Cut three (3) separator samples to 3.0” x 4.0” (76 mm x 102 mm)

5.3.4.2. Weigh each sample in air to the nearest 0.01 g (weight recorded as Dry Weight)

5.3.5. Procedure:

5.3.5.1. Place the samples in a 1 liter beaker and add sufficient 0.1% Aerosol OT solution to
completely cover the samples.

5.3.5.2. Put the beaker with samples in the desiccator and evacuate the desiccator with either a water
aspirator or a vacuum pump.

5.3.5.3. After 4 hours of vacuum, attach each of the samples to the balance and measure its weight in
the aqueous fluid to the nearest 0.01g (weight recorded as Immersed Weight).

5.3.5.4. Remove each sample from the Aerosol solution and wipe away the liquid droplets on the
separator surfaces with a wet cloth.

5.3.5.5. Weigh each damp separator in air to the nearest 0.01g (weight recorded as Damp Weight).

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5.3.6. Calculations:

5.3.6.1. % Volume Porosity = 100(Damp Weight – Dry Weight)/(Damp Weight – Immersed Weight)

5.3.6.2. Calculate the percent volume porosity for each test sample and report as the average of
three determinations.

5.4. Test IV – Determination of Pore Size Distribution

5.4.1. Scope: This method covers the measurement of pore size distribution of battery separator
materials.

5.4.2. Applicable Documents:

5.4.2.1. Superpressure Inc. Aminco Instruction Manual 1160A, (2/76).

5.4.2.2. Quantichrome instruction manual.

5.4.2.3. Micromeretics instruction manual.

5.4.3. Significance and Use:

5.4.3.1. Pore size distribution is a measure of the internal structure of separator materials. A
knowledge of this distribution is essential in the selection of separators for various
applications of batteries.

5.4.3.2. Pore size of materials in the operating instrument range of 100 microns down to .003
microns. 1 micron = .001 mm may be evaluated. Only the open pores of the material which
are accessible from the outer boundaries are measured. Closed cell materials cannot be fully
measured. Cell structures with smaller channels or openings leading to a larger pore opening
will measure and reflect the smaller opening, due to the greater pressure required. Other
useful information is also calculated from the data as follows:

Average Pore Size


Apparent and Real Density
Total Porosity
Percent of Pores Greater than 20 microns

5.4.4. Principle:

Mercury is forced into the open structure of material by increasing pressure form atmospheric
to 60000 psi absolute. The volume of mercury forced into the pores is noted at the various
absolute pressures.

5.4.5. Precautions:

5.4.5.1. Mercury is poisonous. Avoid contact with skin and internal ingestion. Use protective gloves.
Clean up spills immediately with mercury clean-up kits. Keep containers of mercury closed at
all times. When cleaning mercury with mercury cleaning-kit and nitric acid, do so under well
ventilated hood.

5.4.5.2. Disconnect power source before working inside the porosimeter cabinet.

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5.4.5.3. After the 0-5000 psi gauge is cut off at 4000 psi and higher pressurization is continued, be
sure the 0-5000 psi gauge valve is tight and not leaking. If the gauge continues to rise,
stop further pressurization until corrected. Do not allow pressure to exceed 60,000 psi.

5.4.5.4. Keep head and body clear of pressure vessel head during high pressure operation. Be sure
bleed screw is tight before pressurization and that pressure is fully released before removing
bleed nut screw.

5.4.5.5. When reducing high pressure by means of the pressure regulator valve, open the valve very
slowly to prevent hydraulic fluid from flowing too fast into plastic drain bottle. If this is not
done, the hydraulic fluid will overflow causing spillage.

5.4.5.6. Never open the 0-5000 psi gauge valve while high pressure readings are above 4000
psi.

5.4.6. Apparatus:

5.4.6.1. Aminco, 60,000 psi porosimeter, Model J5-7125D, 60K. (In this case, Serial No. K2-1049)
and associated accessories.

5.4.6.2. Quantichrome porosimeter

5.4.6.3. Micromeretics porosimeter

5.4.6.4. A mercury clean-up kit and associated apparatus, Cat. NO. 4439, may be ordered from J. T.
Baker, as well as Cat. No. 09771-10, and may be ordered from Fisher Scientific Co. Copies
of these items and instructions are included in this method.

5.4.6.5. A mercury cleaning apparatus which is Cat. NO. 6440-R10 May be ordered from Thomas.

5.4.6.6. Laboratory exhaust hood, nitric acid and associated glassware and safety goggles, gloves
and protective clothing.

5.4.7. Procedure:

Follow the detailed procedure as outlined in the instruction manual provided with the
instrument

5.4.8. Calculations:

The pore diameter is calculated from the relationship:

D = 175/P, where P is the absolute pressure and 175 is the pore diameter at 1 psia with a
contact angle of 130º and mercury with a surface tension of 473 dynes/cm.

Note: A psia of 6.6 to 14.7 covers the pore size range from 100 to 12 microns. The high
pressure system to 60,000 psia covers the pore size range from 2 down to 0.003 microns.

5.5. Test V – Analyses for Impurities and Acid Extractables

5.5.1. Procedure VA – Acid Extraction

5.5.1.1. Scope: This method covers the method of removal of acid soluble contaminants from a
battery separator for analysis of metal impurities and chlorides.

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5.5.1.2. Apparatus:

5.5.1.2.1. 250 ml Erlenmeyer flask with standard ground glass joint.

5.5.1.2.2. Reflux condenser with joint.

5.5.1.2.3. Thermostat-controlled hot plate.

5.5.1.2.4. Balance capable of weighing to an accuracy of ±0.001 grams.

5.5.1.2.5. Sulfuric Acid (“Baker Instra-Analyzed” for Trace Metal Analysis).

5.5.1.2.6. Distilled Water.

5.5.1.2.7. Scalpel or scissors.

5.5.1.2.8. 500 ml Volumetric flask.

5.5.1.2.9. Filter unit (Nalgene, Catalog #450-0045, with 0.45 micron membrane)

5.5.1.3. Preparation of Reagents

Sulfuric Acid 1.260 specific gravity – to 2 liters of distilled water in a 4 liter Erlenmeyer flask
add 644 ml Sulfuric Acid. Stir, cool to room temperature and adjust specific gravity.

5.5.1.4. Procedure:

5.5.1.4.1. Accurately weigh 10.000 ± 0.010 g of separator material, which has previously been cut into
0.1” x 0.1” squares (0.25 cm x 0.25 cm squares) from various portions of the separator,
including ribs, and dried at 100ºC - 110ºC (212°F – 230°CF)for 1 hour.

5.5.1.4.2. Transfer the weighed material to the 250 ml Erlenmeyer flask and add 150 ml of 1.260 s.g.
Sulfuric Acid.

5.5.1.4.3. Attach reflux condenser, mount on hot plate, bring rapidly to a boil and adjust reflux rate to 1
drop per second.

5.5.1.4.4. After boiling for 3 hours, remove assembly from hot plate and allow to cool to room
temperature.

5.5.1.4.5. Filter the solution through the filter unit with the use of the water aspirator.

5.5.1.4.6. Wash the flask and sample several times with distilled water and transfer the washings to the
filter unit.

5.5.1.4.7. Transfer the filtrate to the 500 ml volumetric flask, washing the filter unit with distilled water,
and dilute to the mark with distilled water.

5.5.1.4.8. This extract is now ready for chloride and/or metal analysis

5.5.2. Procedure VB – Chloride Analysis

5.5.2.1. Scope: This method covers the analysis of leachable chloride form battery separators.

5.5.2.2. Apparatus:

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5.5.2.2.1. Three 10 ml – volumetric flasks, pyrex

5.5.2.2.2. Three 100 ml – volumetric flasks, made of polymethylpentene (PMP)

5.5.2.2.3. One 1000 ml – volumetric flask, pyrex

5.5.2.2.4. Three 25 ml – pipettes

5.5.2.2.5. One 10 ml – dispensette with 1 liter amber color bottle

5.5.2.2.6. One 50 ml – dispensette with 1 gallon plastic bottle

5.5.2.2.7. One centrifuge

5.5.2.2.8. One box – 50 ml disposable centrifuge tube

5.5.2.2.9. One 1000 ml – pipettor with disposable tips

5.5.2.2.10. One 1000 ml – graduated cylinder

5.5.2.2.11. One 4000 ml – Erlenmeyer flask

5.5.2.2.12. One Thermometer – 0ºC - 110ºC (32°C – 230°C)

5.5.2.2.13. One Hydrometer – 1.200 – 1.400 specific gravity range

5.5.2.2.14. One Atomic Absorption Spectrophotometer

5.5.2.2.15. One Ag lamp

5.5.2.2.16. One Source of dry compressed air

5.5.2.2.17. One Cylinder of acetylene

5.5.2.2.18. Nitric Acid – Trace metal analysis grade

5.5.2.2.19. Sulfuric Acid – Trace metal analysis grade

5.5.2.2.20. 1000 ppm silver standard – purchased from J. T. Baker Chemical Company

5.5.2.3. Preparation of Reagents

5.5.2.3.1. Sulfuric Acid 1.260 sp. gr. As prepared in Step 5.5.1.3.

5.5.2.3.2. Silver standard 250 ppm: Pipet 250 ml silver standard of 1000 ppm into a 1000 ml vol. flask
and dilute to mark with glass-distilled, deionized water. Transfer the solution into amber
colored bottle equipped with 10 ml dispensette. Store the bottle in a dark place.

5.5.2.3.3. Nitric Acid (50%) – Dilute 500 ml Nitric Acid to one liter with glass-distilled, deionized water.
Store in amber colored bottle equipped with 10 ml dispensette.

5.5.2.4. Procedure

5.5.2.4.1. Pipet 25 ml of the acid extract from VA into a 100 ml vol. Flask.

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5.5.2.4.2. Add 5 ml 50% Nitric Acid (Reagent 5.5.2.3.3) and 10 ml 250 ppm standard silver solution
(Reagent 5.5.2.3.2).

5.5.2.4.3. Dilute the contents with glass-distilled water to the mark.

5.5.2.4.4. Store the flask in a dark area for 2 – 3 hours.

5.5.2.4.5. Decant 45 – 50 ml supernatant liquid from the flask into centrifuge tube.

5.5.2.4.6. Centrifuge the tube for 15 minutes.

5.5.2.4.7. Pipet 1 ml of this solution into a 10 ml vol. flask and make up the volume with glass-distilled
water.

5.5.2.4.8. Prepare a dilute standard Ag+ solution by pipetting 7.5 ml of 1.260 Sulfuric Acid (Reagent
5.5.2.3.1) into another 100 ml vol. flask and repeating Steps 5.5.2.4.2 to 5.5.2.4.7.

5.5.2.4.9. Prepare a blank by adding 5 ml 50% Nitric Acid and 7.5 ml 1.260 Sulfuric Acid to a 100 ml
vol. flask and repeating Steps 5.5.2.4.3 to 5.5.2.4.8.

5.5.2.4.10. Measure concentration of Ag+ ion in sample (5.5.2.4.7) using the dilute (2.500 ppm) standard
Ag+ solution (5.5.2.4.8) and the blank (5.5.2.4.9) with A.A. spectrophotometer.

5.5.2.5. Calculations:

Amount of leachable chloride in separator = 658(2.500 – X)ppm

Where X = Amount of Ag in ppm found by AA in sample (5.5.2.4.7) as determined in


5.5.2.4.10.

5.5.3. Procedure VC – Metal Analysis

5.5.3.1. Scope: This method covers the determination of leachable trace metal content in battery
separators.

5.5.3.2. Apparatus

5.5.3.2.1. Atomic Absorption Spectrophotometer

5.5.3.2.2. Metal ion standards

5.5.3.2.3. Glassware

5.5.3.3. Procedure:

5.5.3.3.1. Analysis is performed on the acid extract from VA.

5.5.3.3.2. Perform the various metal ion analyses using procedures in the technical literature or those
provided with the AA spectrophotometer.

5.6. Test VI – Stiffness Measurement

5.6.1. Scope: This test indicates the initial stiffness of a separator by measuring the amount of
torque required to flex or deflect a test specimen 15º on both sides of the specimen plane,
with results reported as an average of the two readings.

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5.6.2. Applicable Documents: A more detailed procedure may be purchased from the Technical
Association of the Pulp and Paper Industry, Technology Park/Atlanta, P.O. Box 105113,
Atlanta, GA 30348. Request TAPPI Std. T489 os-76 Stiffness of Paperboard.

5.6.3. Significance and Use: Rigidity of leaf separators is an important factor in the blocking of
elements.

5.6.4. Apparatus:

5.6.4.1. Taber V-5 Model 150-B Tester. Teledyne or equivalent

5.6.4.2. Paper Cutter (Note: a Triple Cut Specimen Shear Model 104-11 is available from Teledyne
Taber, which allows preparation of the test specimen in one stroke).

5.6.5. Test Specimens

5.6.5.1. Conditioning of Samples – samples sensitive to moisture should be conditioned for at least 3
hours in a temperature and humidity controlled room maintained at 50% ± 2% relative
humidity and 73ºF ± 2ºF (22.8°C ± 1.1°C).

5.6.5.2. Specimen Preparation – Cut uniform to size 1-1/2” x 2-3/4” (38 mm x 70 mm). The ribs must
be parallel with the 2-3/4” (70 mm) length and a minimum of 3 ribs included in the specimens.
Also cut another sample to the same dimension, the 2-3/4” (70 mm) length at a right angle to
the ribs.

5.6.6. Preparation of Apparatus:

Level the instrument with the adjustable tips on the front stand legs so that the pendulum
lines up with the zero point.

5.6.7. Procedure:

5.6.7.1. Insert sample with the 2-3/4” dimension in a vertical position, with sample edge facing
operator, between the guide rolls and the clamping jaws such that the top edge of sample is
even with top edge of clamps, and bottom edge rests on plate beneath rollers. Center edge of
sample so that middle is divided in half by the center line above the clamping jaws. Tighten
clamps securely. Adjust rollers so that the bottom portion of sample is centered and makes
contact with the rollers, then back off ¼ turn on each roller adjusting screw. Place appropriate
weight on bottom of pendulum stud for the proper sample stiffness range. Use only the
necessary weight which allows the greatest scale range reading.

5.6.7.2. The stiffness tester is then activated by pushing the switch arm to the right and held in the
”ON” position until the top line on the pendulum lines up with the 15 degree line on the inner
scale mark. When this alignment is reached, immediately read the scale number directly
opposite the outside stationary scale. Note reading and repeat procedure to the left.

5.6.8. Calculations:

5.6.8.1. Average the left and right scale readings.

5.6.8.2. Stiffness (g-cm) = (avg. of scale readings x value stamped on aug. weight)/100

5.6.9. Reporting:

Report stiffness values obtained for samples as rib direction and cross-rib direction.

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5.6.10. Maintenance of Equipment:

Further details about the test instrument may be obtained from the manufacturer. Teledyne
Taber Instrument Corporation, 111 Goundry St., North Tonawonda, NY 14120.

5.7. Test VII – Determination of Puncture Resistance

5.7.1. Procedure VIIA – Globe Tester

5.7.1.1. Scope: This method covers measuring the force required to puncture battery separators.

5.7.1.2. Apparatus:

5.7.1.2.1. Water Receptacle – A one quart (946 ml) can with a flexible wire handle. Diameter of can 4-
1/8 inches (105 mm), height 4-7/8 inches (124 mm).

5.7.1.2.2. Water Reservoir – A metal or plastic container approximately 6-5/8 inches (168 mm) high, 6-
1/4 inches (159 mm) wide, and 13-1/4 inches (337 mm) long.

5.7.1.2.3. Globe puncture tester per attached drawing.

5.7.1.2.4. Balance – A balance with counterweight and 1500 g capacity for the water receptacle.

5.7.1.2.5. Paper Cutter – Paper cutter to be use in cutting sample to size.

5.7.1.3. Test Specimens:

5.7.1.3.1. Test specimens are obtained by cutting a 1-1/2 inch to 2 inch section from a separator. Cut
parallel to the ribs at a location that will permit puncture of the web but no contact with ribs.

5.7.1.3.2. A minimum of six separators should be tested.

5.7.1.3.3. To obtain wet puncture, submerge the specimen in water and puncture while wet.

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5.7.1.4. Preparation of Apparatus:

5.7.1.4.1. Fill the receptacle with water and hang in place on the puncture tester lever locating the wire
handle in the notch. Block the lever so that it is parallel with the puncture tester base. The
distance from point of contact of wire/lever and the center of the bottom of the can (inside)
should be 8-3/8 inches ± 1/32 inch (213 mm ± 1 mm).

5.7.1.4.2. Base of reservoir is located three feet above base of puncture tester.

5.7.1.4.3. The container is fitted with an inlet pipe which is connected to a tap water source. A float
arrangement controls addition of water to maintain water level in the tank at approximately 4-
1/2 inches (114 mm).

5.7.1.4.4. An outlet pipe is fitted into one end of the tank just above the tank bottom.

5.7.1.4.5. The outlet pipe has a valve just outside the tank.

5.7.1.4.6. The shutoff valve is connected to a solenoid which is controlled by a snap micro switch/relay.
This is the start switch for the circuit.

5.7.1.4.7. Automatic shutoff of water flow is accomplished by means of a third micro switch which is
located under the lever in such a position that it is triggered by the dropping lever at the
moment of sample puncture.

5.7.1.4.8. A ¼ inch I.D. rubber tube directs water flow from the solenoid to the water receptacle. The
outlet end of this tube has a metal tip with a .089 inch orifice.

5.7.1.4.9. A standard grease fitting with .089 inch hole makes an ideal tip. The water dispensing tip is
positioned approximately 4 inches above the water receptacle and is held in place by means
of a ringstand with clamp.

5.7.1.4.10. All electrical units are waterproof.

5.7.1.5. Procedure:

5.7.1.5.1. Arrange the test apparatus as described in 5.7.1.4.1 – 5.7.1.4.10.

5.7.1.5.2. Allow the water reservoir to fill to proper level and run water through the solenoid and tube for
a few minutes to purge air from the system.

5.7.1.5.3. Check flow rate by weighing the amount of water dispensed in one minute. Weight of water
dispensed in one minute should be 750 g ± 20 g. If flow rate is outside these limits, the most
probable reason is restriction of flow due to foreign particles in solenoid tubing or dispensing
tip. Clean and recheck the flow rate.

5.7.1.5.4. Slide test specimen between the two holding plates under the puncture pin, locating the
specimen so that the puncture pin will contact web area only. Error will result if the pin
contacts rib material.

5.7.1.5.5. Tighten two opposite corner set screws to prevent sample form shifting.

5.7.1.5.6. Hang the water receptacle from the lever locating the handle in the notch. Using the coarse
and fine counterweight adjustments, balance the lever so that the puncture pin just makes
contact with the specimen but does not exert pressure on it.

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5.7.1.5.7. Position the water reservoir outlet tube approximately 4 inches above the water receptacle.
Push the “start” button. When sufficient water has collected in the receptacle, the puncture
pin will break through the separator’s web, allowing the dropping lever to contact the shutoff
switch which instantly stops the flow of water.

5.7.1.5.8. Transfer the water receptacle to the balance and weigh to the nearest gram. The weight of
water and receptacle minus the receptacle weight is recorded as grams to puncture “dry”. If a
wet puncture is desired, remove the dry punctured specimen and submerge in water
contained in a suitable sized beaker. Allow the specimen to wet thoroughly. Repeat 5.7.1.5.4
– 5.7.1.5.8 and record the weight of water collected as grams to puncture “wet”.

5.7.1.5.9. Allow all water to drain from system after test series has been completed. Store metal water
dispensing tip in oil when not in use.

5.7.2. Procedure VIIB – GNB (“Gould”) Puncture Tester

5.7.2.1. Apparatus:

5.7.2.1.1. Gould National Puncture Tester with water collecting container and counter weight (see
attached drawings).

5.7.2.1.2. Water supply controlled at 750 grams per minute flow rate.

5.7.2.1.3. Stopwatch.

5.7.2.1.4. Balance.

5.7.2.2. Procedure:

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BCIS-02 Rev. Feb02

5.7.2.2.1. Cut separator sample to be tested parallel to the ribs into a strip 1-1/2 inches wide such that
each sample will retain one (1) backweb span and two (2) adjoining ribs.

5.7.2.2.2. Set up the puncture tester and water collecting container as shown in the drawing and
balance the pivot arm with the counterweight.

5.7.2.2.3. Position the separator strip in the holder with the ribs up, allowing the pin to contact only the
backweb. Clamp into position.

5.7.2.2.4. Start water flow into the collecting container maintaining a steady flow of 750 cc/minute. Stop
flow when separator has been completely punctured.

5.7.2.2.5. Weigh and record to the nearest 0.1 gram the water required to puncture the test sample.

5.7.2.2.6. Repeat 5.7.2.2.3 through 5.7.2.2.5 four times for each sample and average the results.

5.8. Test VIII – Wetting Properties

5.8.1. Procedure VIIIA – Acid Flotation Method

5.8.1.1. Scope: This method defines separator wetability in terms of the time required for acid to wick
through the backweb section of the specimen, when it is placed horizontally on the surface of
the acid.

5.8.1.2. Apparatus:

5.8.1.2.1. A glass or other acid resistant tray of dimensions approximately 6” x 6” x 2” (152 mm x 152
mm x 51 mm)for a standard test specimen, or larger for full size separators.

5.8.1.2.2. Stop watch with second hand.

5.8.1.2.3. Sulfuric Acid, 1.265 ± 0.015 specific gravity (80ºF/80°F (26.7°C/26.7°C)).

5.8.1.2.4. Cutting board.

5.8.1.3. Test Specimens:

Cut Samples to 2” x 2” (51 mm x 51 mm) for standard size specimens or use a larger size or
full size separator if desired.

5.8.1.4. Procedure:

5.8.1.4.1. Fill tray with acid to a depth of approximately 1” (25.4 mm).

5.8.1.4.2. Ensure that the test pieces are completely flat.

5.8.1.4.3. Hold the specimen as horizontally as possible, ribs up, and close to the surface of the acid.

5.8.1.4.4. Carefully drop the specimen onto the surface of the acid and start the watch.

5.8.1.4.5. Stop the watch when the top surface of the sample is completely wet with acid. This is usually
noted by a darkening of the surface.

5.8.1.4.6. Record the time and note any incomplete or spotty wetting.

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BCIS-02 Rev. Feb02

5.8.2. Procedure VIIIB – Acid Drop Absorption Method

5.8.2.1. Scope:

This method defines separator wetability in terms of the time required for a drop of acid to be
completely absorbed by the backweb of a separator.

5.8.2.2. Apparatus:

5.8.2.2.1. Automatic Buret, Three-Way, with Teflon Plug, 10 ml capacity (Kimble 17124F or equivalent).

5.8.2.2.2. Support Jack with vertical lift to 10” (VWR Standard Model Cat. #60142-546 or equivalent).

5.8.2.2.3. Stop watch with a second hand.

5.8.2.2.4. Sulfuric Acid, 1.265 ± 0.015 specific gravity (80ºF/80°F (26.7°C/26.7°C)).

5.8.2.2.5. Acid resistant covering for support jack.

5.8.2.3. Test Specimens: Cut separator test specimen to 6” x 6” (152 mm x 152 mm) or smaller.

5.8.2.4. Procedure:

5.8.2.4.1. Place specimen, backweb side up (ribs down), on support jack.

5.8.2.4.2. Move the support jack next to the buret.

5.8.2.4.3. Raise the support jack so that the backweb of the test specimen is exactly 1.0 inch (25.4 mm)
below the top of the buret.

5.8.2.4.4. Deliver a 0.05 ml drop of acid to the specimen surface and immediately start the watch.

5.8.2.4.5. Stop the watch when the drop is completely absorbed, as evidenced by the disappearance of
the shiny surface.

5.8.2.4.6. Record the elapsed time.

5.8.3. Procedure VIIIC – Dry Charge Process Simulation

5.8.3.1. Scope: This test is used to measure the rewetting properties of leachproof separators and flat
sheets.

5.8.3.2. Significance and Use: The test simulated a dry charge procedure in which the separators are
washed in cold water.

5.8.3.3. Apparatus:

5.8.3.3.1. Empty 12 volt battery case.

5.8.3.3.2. Constant temperature water bath at 150ºF ± 5ºF (65.6°C ± 2.8°C).

5.8.3.3.3. Sulfuric acid 1.100 ± 0.005 specific gravity.

5.8.3.3.4. Sulfuric acid 1.250 ± 0.015 specific gravity.

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BCIS-02 Rev. Feb02

5.8.3.3.5. Forced draft oven set at 250ºF ± 10ºF (121.1°C ± 5.6°).

5.8.3.3.6. PVC corrugated liners.

5.8.3.3.7. Glass trays 10” x 10” (254 mm x 254 mm) or larger.

5.8.3.3.8. Stop watch.

5.8.3.3.9. Five gallon perforated pail for washing, including perforated aluminum spacer to hold
samples vertical and away from the bottom of the washing pail.

5.8.3.4. Test Specimens: Sample size is 5-1/2 inches x 5-1/2 inches (140 mm x 140 mm).

5.8.3.5. Procedure:

5.8.3.5.1. Place 10 separators or flat sheets in each cell of the battery, separating each separator with a
corrugated PVC liner.

5.8.3.5.2. Fill each cell with approximately 900 ml of 1.100 specific gravity acid. Acid must be 70ºF ±
5ºF (21.1°C ± 2.8°C) when introduced into the cell. Separators must be covered by the acid.

5.8.3.5.3. Cover the battery case with polyethylene and place in 150ºF (65.6°C) constant temperature
bath for 2-1/2 hours.

5.8.3.5.4. Following the soak, dump the acid and insert separators and PVC liners (separator ribs
vertical) into the pail between the aluminum spacers. The spacers should hold the separators
firmly but not tightly in place. Wash water temperature should be 40ºF ± 5ºF (4.4°C ± 2.8°C).
The flow rate should be adjusted to approximately 7600 ml (2 gallons) per minute. The
separators wash for one hour. Do not wash more than 40 separators at one time. Wash
different wetting systems in different pails.

5.8.3.5.5. The washed separators are removed from the pail and dried (ribs up on the shelf) in the
forced draft oven at 250ºF ± 10ºF (121.1°C ± 5.6°C) for 30 minutes.

5.8.3.5.6. After drying, the separators are allowed to stand at room temperature for at leas ½ hour,
thereby reaching equilibrium moisture. 5 of the samples are rewet in 80ºF (26.7°C) 1.250
specific gravity sulfuric acid. 5 are rewet in 30ºF (-1.1°C) sulfuric acid which is 1.250 specific
gravity at 80ºF (26.7°C) reference point. Samples are floated on the acid (ribs up) and the
time to rewet is measures.

5.8.3.6. Reporting:

Report time to 90% and 100% rewet in seconds. The average and range for each acid
temperature is reported.

6. SEALING COMPOUND

6.1. The sealing compound used on batteries shall meet the performance requirements listed
below or shall enable the battery to meet the following performance requirements. The
sealing compound shall be acid resistant.

6.2. Vibration Test

For two (2) hours, the fully charged battery shall be subjected to a vibration consisting of a
harmonic motion having a frequency of 1900 to 2100 cycles per minute through an amplitude

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BCIS-02 Rev. Feb02

of 0.045” to 0.050” (1.135 mm to 1.270 mm), excursion 0.090” to 0.100” (2.286 mm to 2.540
mm). At the start of the vibration test, the battery temperature shall be 80º ±10ºF (26.7º ±
5.6ºC) and shall be discharged at approximately 1% of the cranking test rate rounded to the
nearest whole number during the vibration test. It must maintain a steady voltage and current,
and at the end of this test, there shall be no adhesion or cohesion failures of the sealing
compound.

6.3. Hot and Cold Cycle Test

The battery must pass ten (10) cycles of 16 hours at 0ºF ± 1ºF (-17.8ºC ± 0.6ºC) and 8 hours
at 70ºF - 90ºF (21ºC - 32ºC) with no signs of cracking or loss of adhesion becoming apparent.
At the 3rd, 6th and 10th cycles, air pressure of one pound per square inch will be applied to
each cell individually, immediately after removing from the cold chamber. This pressure must
be maintained for 15 seconds. In addition to maintaining the air pressure throughout the test,
there shall be no evidence of apparent cohesive cracks.

7. ELECTROLYTE

7.1. Electrolyte shall be a solution of sulfuric acid in pure water at the specific gravity required by
the procuring agency. The capacity and performance requirements though are based on the
electrolyte gravity of 1.265 ± .005 regardless of the gravity at which the batteries are used in
service.

The first-class sulfuric acid used in preparing this electrolyte shall conform to the
requirements of the latest issue of Federal Specifications O-S-801-e, November 21, 1990.

Electrolyte used for filling dry-charged batteries shall conform to the specification which is
quoted below:

7.2. Scope:

This specification covers sulfuric acid electrolyte for use in dry-charged storage for use in dry-
charged storage batteries within a specific gravity range of 1.200 to 1.300 sp. gr. At 80ºF
(26.7ºC).

7.3. Requirements:

7.3.1. The specific gravity of the electrolyte shall be as ordered with a tolerance of ± .003

7.3.2. Specific gravity shall be determined by a hydrometer calibrated at 80ºF/80ºF (26.7ºC/26.7ºC).

7.3.3. The H2SO4 content shall coincide with specific gravity (±.12%).

7.3.4. Impurities in the electrolyte shall not exceed the maximum limits shown in the table below:

Impurity Maximum Limit Percent


per Weight
Organic Matter To pass test defined in Federal Specification
O-S-801-e, Nov. 21, 1990
Fixed Residue 0.03
Iron (Fe) 0.005
Sulfurous Acid (SO2) 0.004
Arsenic (As) 0.0001
Antimony (Sb) 0.0001

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BCIS-02 Rev. Feb02

Manganese (Mn) 0.00002


Nitrates (NO3) 0.0445
Ammonium (NH4) 0.001
Chloride (Cl) 0.001
Copper (Cu) 0.005
Zinc (Zn) 0.004
Selenium (Se) 0.002
Nickel (Ni) 0.0001
Platinum (Pt) To pass test defined in Federal Specification
O-S-801-e, 1990

8. INTERCELL CONNECTORS

Intercell connectors shall be of the “burned-on” type, or the equivalent. The voltage drop in
the intercell connectors shall not exceed 20 millivolts per inch (0.79 mV/mm) of distance
between post centers when discharging at 300 amperes*, the battery and connectors being
at 80ºF (26.7ºC). Intercell connectors shall not obstruct the filling apertures.

*150 amperes for 12 volt batteries below 180 minutes in Reserve Capacity.

9. POST STRAPS

Post straps shall be of lead-antimony alloy (not for VRLA batteries). Plates of like polarity in
each cell shall be integrally “burned” to the respective straps. Straps shall be of adequate
design, size and strength to be adequate electrical conductors and supports for the group of
plates.

10. PLATES

The plates used in constructing batteries covered by this specification shall be of the size,
number and thickness that will enable the battery to meet its electrical performance rating
requirements.

11. HANDLES

Attached metal handles, when used, shall be of good quality steel, covered with an acid-
resisting coating and securely attached to the ends of containers. Such handles shall not
increase the dimensions of batteries over the limits specified. Acid resistant cordage is
another approved material for handles.

12. TAPERED TERMINAL POSTS

Tapered terminal posts shall have dimensions as follows:

Inches Millimeters
Small 5/8 15.88
diameter of
negative
posts
Small 11/16 17.47

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BCIS-02 Rev. Feb02

diameter of
positive posts
Taper per foot 11/32 33.87
Minimum 5/8 15.88
length of
taper

13. SIDE TERMINALS

Side terminals are located on side of battery container as shown in figure 17 of “BCI
Assembly Numbers, Cell Layouts, and Terminals” table of the BCI replacement data book.
The positive terminal shall be indicated by Pos., P, or + on the cover near the terminal boss.
Both positive and negative terminals are designed to receive a 3/8-16UNC-2B and threaded
screw, which must not enter over 0.34” (8.6 mm) into case.

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